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Diethanolamine → 2-[Bis-(2-hydroxyethyl)-amino]-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

HRID 345998
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 345998
[NH:1]([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4].[OH-].[Na+].Cl[C:11]1[N:16]=[C:15]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[N:14]=[C:13]([N:23]2[C:28]([CH3:30])([CH3:29])[CH2:27][C:26]3([O:34][CH2:33][CH2:32][O:31]3)[CH2:25][C:24]2([CH3:36])[CH3:35])[N:12]=1>O.C1(C)C(C)=CC=CC=1>[OH:4][CH2:3][CH2:2][N:1]([CH2:5][CH2:6][OH:7])[C:11]1[N:16]=[C:15]([N:17]2[CH2:18][CH2:19][O:20][CH2:21][CH2:22]2)[N:14]=[C:13]([N:23]2[C:24]([CH3:36])([CH3:35])[CH2:25][C:26]3([O:31][CH2:32][CH2:33][O:34]3)[CH2:27][C:28]2([CH3:30])[CH3:29])[N:12]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 8113Diethanolamine2×HCID 14798Sodium Hydroxide2×HCID 199917602-Chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine2×

Produkt 1

HCID 199917692-[Bis-(2-hydroxyethyl)-amino]-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
2×
HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

5.3 g of diethanolamine and a solution of 1 g of NaOH in 3 ml of water are added to a solution of 20 g of 2-chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (product from Example 44) in 50 ml of xylene. 1 g of NaOH in 3 ml of water is again added after 1.75 hours with stirring under reflux. After 14 hours, 7.9 g of diethanolamine are added, after which the mixture is stirred under reflux for a further 28 hours. It is then allowed to cool and washed with water, and the organic phase is separated off. After drying over Na2SO4, evaporating and recrystallizing twice from toluene, the above product is obtained as a white powder which melts at 135°-140°.

Aufarbeitung

  1. temperatureunder reflux
  2. stirringafter which the mixture is stirred
  3. temperatureunder reflux for a further 28 hours
  4. temperatureto cool
  5. washwashed with water
  6. customthe organic phase is separated off
  7. dry with materialAfter drying over Na2SO4
  8. customevaporating
  9. customrecrystallizing twice from toluene
  10. customthe above product is obtained as a white powder which melts at 135°-140°

Quellen und Nachweise

ORD-Eintrag
ord-ef585ad905df4281a6974dd7c49ff092
Quelldatensatz
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05059689

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